Zheng Ze-Ke, Ma Xiao-Hong, Zhao Hua-Feng, Yu Le, Zhang Min, Liao Yan-Biao
Department of Electronic Engineering, Tsinghua University, Beijing 100084, China.
Guang Pu Xue Yu Guang Pu Fen Xi. 2009 Dec;29(12):3383-7.
In the present work, spatial character of emission spectrum was analyzed, the effect of laser energy and samples at tribute on the best detection position for the highest signal-to-noise ratio was studied, and some experimental investigations with LIBS technique to detect trace Cu in polluted soil were carried out in our laboratory. A Q-switched Nd : YAG laser operating at 1 064 nm with pulse width of 10 ns and repetition frequency of 1 Hz was utilized. The laser pulse was focused by lens with focal length of 10 cm to generate microplasmas on the surface of printed circuit board and soil samples. The sample was adjustable by vernier construction to detect the emission spectrum of the microplasmas from different position. Experiments showed that the intensity of thermal radiation and atomic radiations evolved differently while the detection position changed. It was verified that thermal radiation reduced rapidly with the distance from the center of spark increasing, while the intensity of atomic radiations increased firstly and decreased after intensity maximum was reached. The method of separating thermal radiation and atomic radiations in space brought on high signal-to-noise ratio. It was found that the best detection position was 0.75 mm off the center of the spark for soil sample while the laser energy was 40 mJ, and the distance increased with the growth of laser energy. With Cu 324.75 nm and Cu 327.39 nm as the analysis lines, the best detection position was selected to detect trace Cu pollution in soil. Internal standard method was used to determine the relation between Cu concentration and its intensity. It was concluded that the detection limit of Cu in soil was 67 mg x kg(-1), which is below the trace element thresholds for Class 2 soil defined in the Environmental Quality Standard for Soil in China. It was proven an effective way to achieve higher signal-to-noise ratio by adjusting the location of spectral measurements. This method was viable for trace Cu detection in polluted soil.
在本工作中,分析了发射光谱的空间特性,研究了激光能量和样品属性对最高信噪比最佳检测位置的影响,并在我们实验室开展了一些利用激光诱导击穿光谱(LIBS)技术检测污染土壤中痕量铜的实验研究。使用了一台调Q Nd:YAG激光器,其工作波长为1064 nm,脉冲宽度为10 ns,重复频率为1 Hz。激光脉冲通过焦距为10 cm的透镜聚焦,以在印刷电路板和土壤样品表面产生微等离子体。样品可通过游标结构进行调节,以检测来自不同位置的微等离子体的发射光谱。实验表明,随着检测位置的变化,热辐射强度和原子辐射强度的变化情况不同。证实了热辐射随着与火花中心距离的增加而迅速降低,而原子辐射强度先增加,在达到强度最大值后降低。在空间上分离热辐射和原子辐射的方法带来了高信噪比。发现当激光能量为40 mJ时,土壤样品的最佳检测位置是距离火花中心0.75 mm处,并且该距离随着激光能量的增加而增大。以Cu 324.75 nm和Cu 327.39 nm作为分析谱线,选择最佳检测位置来检测土壤中的痕量铜污染。采用内标法确定铜浓度与其强度之间的关系。得出土壤中铜的检测限为67 mg·kg⁻¹,低于中国《土壤环境质量标准》中规定的二级土壤微量元素阈值。证明了通过调整光谱测量位置来实现更高信噪比是一种有效的方法。该方法对于污染土壤中痕量铜的检测是可行的。